CN104402533A - Method for vacuum cladding of metal coating layer on silicon carbide surface - Google Patents
Method for vacuum cladding of metal coating layer on silicon carbide surface Download PDFInfo
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- CN104402533A CN104402533A CN201410564436.3A CN201410564436A CN104402533A CN 104402533 A CN104402533 A CN 104402533A CN 201410564436 A CN201410564436 A CN 201410564436A CN 104402533 A CN104402533 A CN 104402533A
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- silicon carbide
- mixed powder
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Abstract
The invention discloses a method for vacuum cladding of a metal coating layer on a silicon carbide surface, and belongs to the ceramic material technical field. The method is carried out by the following steps: preparation of a metal mixed powder (weighing, mixing, ball milling, drying and sieving), preparation of a paste, and ceramic surface coating and vacuum cladding. The metal mixed powder comprises the components by the mass percentage: 10-40% of Mo, 18-32% of Ni or Co, and 36-70% of Si; the vacuum cladding temperature is 1300-1400 DEG C, and the vacuum cladding time is 10-30 min. The method can be used as a preparation process of a transition layer for soldering silicon carbide with metals, the prepared coating layer can significantly improve the wettability between the metals and silicon carbide, an overreaction in the soldering process of silicon carbide ceramics and a soldering material is reduced or prevented, so as to improve the bonding strength of a ceramic/metal soldered interface.
Description
Technical field
The present invention relates to a kind of preparation method of silicon carbide metallic coating, particularly adopt vacuum cladding technology to prepare the method for metallic coating at silicon carbide, object is the wettability improving metal pair silicon carbide ceramics, belongs to technical field of ceramic material.
Background technology
Silicon carbide has excellent mechanical property, high thermal conductivity and good thermal shock resistance etc., and these characteristics make them in aerospace, is used widely in the field such as automotive industry and the energy.But the shortcoming of silicon carbide ceramics poor toughness, processing difficulties limits its application, and metal has excellent plasticity, toughness and good processibility, but the high-temperature behavior of most of metal and alloy thereof is poor, if the two to be combined the advantage giving full play to them, very outstanding structure-function integration material will be formed.The interconnection technique of silicon carbide and metal is the gordian technique that the larger application of silicon carbide acquisition must solve.Soldering is connected material by the solder wetting of fusing and is formed joint, and in connection procedure, be connected mother metal can keep non-fusible, and therefore soldering is differing greatly for switching performance and to the advantage having its uniqueness during the material that fusing is responsive.Make like this at high technology ceramics with pottery, Ceramic and metal joining technology, method for brazing is most important method of attachment.For Ceramic brazing, it is the prerequisite realizing connecting that the Small angle of solder to pottery soaks.
SiC ceramic is the compound that a kind of covalency key is very strong, shows highly stable electron coordinate.The basic structural unit of its crystalline structure is SiC
4and CSi
4coordination tetrahedron, is combined by the strong tetrahedron sp bond of orientation, and has polarization to a certain degree.The ion key of the electronegativity of Si to be the electronegativity of 1.8, C be 2.6, Si-C key only accounts for 12%.Huge difference is there is in SiC pottery and metallic substance in process based prediction model, cause SiC pottery be difficult to do not added the liquid metal of interfacial activity metallic element (as Ti, Cr) or alloy institute soak, this be affect SiC Ceramic brazing connection essential problem.And by preparing metallic coating to silicon carbide, make liquid metal and the wetting of SiC become soaking between liquid metal and metallic coating, thus significantly improve the wettability of metal or alloy melt and SiC pottery, very favourable to the soldering of SiC and metal.
Metallic coating method is formed about thyrite surface, the main of current application and research is exactly by plating, electroless plating or immersed method etc. at SiC ceramic surface formation metal level, as Chinese patent ZL200710035759.3 " a kind of high-performance ceramic surface metallization process " forms metal layer by electroplating and burning nickel at material surface; Chinese patent ZL200510029905.2 " SiC ceramic particle surface electroless copper plating method " and ZL200510029906.7 " SiC ceramic particle surface tangsten plating process " utilizes the method for electroless plating to carry out electroless copper and the process of plating tungsten to ceramic grain surface; Chinese patent ZL200410012575.1 " surface alloying ceramic and preparation method " utilizes composition target to carry out Alloying Treatment to ceramic material surfaces; Chinese patent 200910092748.8 method of attachment of metal " pottery with " is carrying out allowing ceramic surface adhere to one deck aluminum or aluminum alloy film to carry out surface treatment to stupalith by being immersed by pottery in aluminum or aluminum alloy liquation in ceramics-to-metals joining process.But, the metallic diaphragm that these SiC ceramic or particle surface are formed, or in conjunction with undertighten, or follow-up heat treatment process can react with silicon carbide substrate, or can not use in high temperature occasion.
In addition, Chinese patent 201310140262.3 " a kind of method improving metal pair SiC ceramic wettability " is the method adopting the metal ion of ion implantation doses in surface of SiC, improves the wettability of metal on SiC.Chinese patent 201310392098.5 " a kind of side metallization of silicon carbide ceramics and method for metallising " is by being carried out sintering by the mixed powder of pottery (TiC or WC or the mixture both it), Co, Si and B or the method for plasma spraying, preparing metal+ceramic composite coating in SiC ceramic surface.Chinese patent ZL201110211637.1 " SiC ceramic surface treatment method and uses thereof " is then by applying TiH in surface of SiC
2paste, after vacuum heat treatment, forms one in surface of SiC and has metallic Ti (C, Si) composite ceramic coat.
Summary of the invention
The object of the invention is the preparation method providing a kind of silicon carbide ceramics surface superior metal coating, namely form by vacuum cladding the metallic coating that one deck has metallicity, high-temperature stability and bonding strength on silicon carbide ceramics surface, and obvious surface reaction does not occur for coating and silicon carbide substrate, to improve the wettability of metal pair silicon carbide ceramics.
The present invention takes following technical scheme to be achieved, a kind of method of silicon carbide ceramics surface vacuum deposited metals coating, carries out according to following step:
1) Mo, Ni or Co and Si powder are carried out weighing, mixing than composition by certain mass, in tumbling ball mill, with sintered carbide ball or agate ball for abrading-ball, alcohol is ball-milling medium, and metal mixed powder is made in ball milling >=24 hour;
2) above-mentioned metal mixed powder is placed in 80 DEG C of vacuum drying ovens to dry, and crosses 200 mesh sieves;
3) get the metal mixed powder that the above-mentioned mistake of part is sieved, add appropriate organic binder bond, after fully stirring, obtain even paste;
4) paste is covered the silicon carbide ceramics of clean on the surface by brushing or method for printing screen by hand;
5) by the silicon carbide ceramics sheet of coating, vacuum oven (vacuum tightness≤4 × 10 are placed in
-2pa), be heated to certain temperature with≤10 DEG C/min, held for some time, make the complete cladding of metal mixed powder at ceramic surface, then be cooled to room temperature with≤5 DEG C/min, form fine and close metallic coating.
The certain mass number of wherein said Mo, Ni or Co and Si powder consists of:
Mo:10 ~ 40 part, Ni or Co:18 ~ 32 part, Si:36 ~ 70 part.
Described binding agent is Terpineol 350+ethyl cellulose solution, and Terpineol 350: ethyl cellulose: metal mixed powder=9g:1g:10g.
Described vacuum cladding temperature is 1300 ~ 1400 DEG C, and soaking time is: 10 ~ 30 min.
The present invention has the features such as vacuum cladding process system operation is few, and temperature range is wide, and conforming product rate is high, and production cost is low, applicable large-scale production; It is even that metallic coating has thickness, and dense structure, with substrate combinating strength advantages of higher.
Accompanying drawing explanation
Fig. 1 is 1 and No. 2 sample photomacrograph (be contrast coatingsurface color, add uncoated SiC ceramic sample photo) in embodiment.
Fig. 2 be in embodiment No. 1 sample (metallic coating consists of 10Mo+20Co+70S
i) section (a) and Cu be the wetting photo (b) of this No. 1 specimen surface.
Fig. 3 is No. 2 sample (metallic coating consists of 20Mo+18Co+62Si) sections (a) and the wetting photo (b) of Cu at these No. 2 specimen surfaces in embodiment.
Embodiment
Below in conjunction with specific embodiment 1-5, the present invention is further elaborated.The certain mass percent of Mo, Ni or Co of the present invention and Si powder consists of: the Mo of 10 ~ 40%, Ni or Co of 18 ~ 32%, the Si of 36 ~ 70%.
Appropriate binding agent of the present invention is Terpineol 350+ethyl cellulose solution, and Terpineol 350: ethyl cellulose=9g:1g:10g.
Described vacuum cladding temperature is 1300 ~ 1400 DEG C, and soaking time is: 10 ~ 30 min.
A method for silicon carbide ceramics surface vacuum deposited metals coating, the method is made up of following steps:
1) commercially available Mo, Ni or Co and Si powder undertaken weighing, mixing by certain mass percent composition, in tumbling ball mill, with sintered carbide ball or agate ball for abrading-ball, alcohol is ball-milling medium, and metal mixed powder is made in ball milling >=24 hour;
2) above-mentioned metal mixed powder is placed in 80 DEG C of vacuum drying ovens to dry, and crosses 200 mesh sieves;
3) get the metal mixed powder that above-mentioned mistake is sieved by part, add appropriate organic binder bond, after fully stirring, obtain even paste;
4) paste is covered the silicon carbide ceramics of clean on the surface by brushing or method for printing screen by hand;
5) by the silicon carbide ceramics sheet of coating, vacuum oven (vacuum tightness≤4 × 10 are placed in
-2pa), be heated to certain temperature with≤10 DEG C/min, held for some time, make the complete cladding of metal mixed powder at ceramic surface, then be cooled to room temperature with≤5 DEG C/min, form fine and close metallic coating.
embodiment 1-5
1) undertaken weighing, mixing by the formula of table 1 by commercially available Mo, Ni, Co and Si powder, in tumbling ball mill, with sintered carbide ball or agate ball for abrading-ball, alcohol is ball-milling medium, and metal mixed powder is made in ball milling >=24 hour, specifically fills a prescription in table 1;
Table 1 metallic coating formula
2) above-mentioned metal mixed powder is placed in 80 DEG C of vacuum drying ovens to dry, and crosses 200 mesh sieves;
3) get the metal mixed powder that above-mentioned mistake is sieved by part, add appropriate Terpineol 350+ethyl cellulose solution (Terpineol 350: ethyl cellulose: metal mixed powder=9g:1g:10g), after fully stirring, obtain even paste;
4) paste is covered the silicon carbide ceramics of clean on the surface by coating or method for printing screen by hand;
5) by the silicon carbide ceramics sheet of coating, vacuum oven (vacuum tightness≤4 × 10 are placed in
-2pa), be heated to 1300 ~ 1400 DEG C with≤10 DEG C/min, insulation 10 ~ 30 min, make the complete cladding of metal mixed powder at ceramic surface, then are cooled to room temperature with≤5 DEG C/min, form fine and close metallic coating (Fig. 1 is 1 and No. 2 sample photomacrograph).Coating method and the melting and coating process of sample are as shown in table 2;
The coating method of table 2 sample and melting and coating process
| Numbering | Vacuum cladding temperature (DEG C) | Soaking time (min) | Coating method |
| 1 | 1350 | 30 | Silk screen printing |
| 2 | 1350 | 30 | Silk screen printing |
| 3 | 1300 | 20 | Manual application |
| 4 | 1350 | 30 | Manual application |
| 5 | 1400 | 10 | Silk screen printing |
6) silicon carbide ceramics will metallized, with diamond saw blade along cutting perpendicular to coating direction, after polishing polishing, under scanning electron microscope, observe the thickness of coating and the thickness of matrix and coating and coating structure pattern (wherein Fig. 2 a and Fig. 3 a is the section of 1 and No. 2 sample).Be coated with layer microstructure test result as shown in table 3;
Table 3 is coated with layer microstructure test result
| Numbering | Microstructure | Metallization layer thickness (μm) | Coating/basal body interface reaction |
| 1 | Evenly, fine and close | 30~40 | Without sharp interface responding layer |
| 2 | Evenly, fine and close | 20~30 | Without sharp interface responding layer |
| 3 | Evenly, fine and close | 30~40 | Without sharp interface responding layer |
| 4 | Evenly, fine and close | 10~20 | Without sharp interface responding layer |
| 5 | Evenly, fine and close | 20~30 | Without sharp interface responding layer |
7) wetting angle of high-temperature moisture testing of equipment Cu and Al on different metal ceramic substrate surface is adopted.For Cu, test condition is: 1120 ° of C, be incubated 15 min, heat-up rate 5 ° of C/ minute, and vacuum tightness is 4 × 10
-4pa.For Al, test condition is: 900 ° of C, be incubated 15 min, heat-up rate 5 ° of C/ minute, and vacuum tightness is 4 × 10
-4.The wetting angle test result of two kinds of pure metal on different metal pottery is as shown in table 4.Wherein Fig. 2 b and Fig. 3 b is Cu and the wetting photo at 1 and No. 2 specimen surface.
The wetting angle of table 4 two kinds of pure metal on different metal SiC ceramic specimen surface
| Numbering | Wetting angle (Cu) | Wetting angle (Al) |
| 1 | 14o | 8o |
| 2 | 7o | 39o |
| 3 | ? | 0o |
| 4 | ? | 15o |
| 5 | ? | 37o |
The present invention is not limited to above-mentioned specific embodiments, and above-mentioned specific embodiments is only schematic, guiding instead of restrictive.The present invention can be follow-up with embodiment the integrated process such as soldering, Electronic Packaging use.
Claims (5)
1. a method for silicon carbide ceramics surface vacuum deposited metals coating, is characterized in that carrying out according to following step:
1) Mo, Ni or Co and Si powder are carried out weighing, mixing than composition by certain mass, in tumbling ball mill, with sintered carbide ball or agate ball for abrading-ball, alcohol is ball-milling medium, and metal mixed powder is made in ball milling >=24 hour;
2) above-mentioned metal mixed powder is placed in 80 DEG C of vacuum drying ovens to dry, and crosses 200 mesh sieves;
3) get the metal mixed powder that the above-mentioned mistake of part is sieved, add appropriate organic binder bond, after fully stirring, obtain even paste;
4) paste is covered the silicon carbide ceramics of clean on the surface by brushing or method for printing screen by hand;
5) by the silicon carbide ceramics sheet of coating, be placed in vacuum oven, be heated to certain temperature with≤10 DEG C/min, held for some time, make the complete cladding of metal mixed powder at ceramic surface, then be cooled to room temperature with≤5 DEG C/min, form fine and close metallic coating.
2. the method for a kind of silicon carbide ceramics surface vacuum deposited metals coating according to claim 1, it is characterized in that the certain mass number of described Mo, Ni or Co and Si powder consists of: Mo:10 ~ 40 part, Ni or Co:18 ~ 32 part, Si:36 ~ 70 part.
3. the method for a kind of silicon carbide ceramics surface vacuum deposited metals coating according to claim 1, is characterized in that described binding agent is Terpineol 350+ethyl cellulose solution, and Terpineol 350: ethyl cellulose: metal mixed powder=9g:1g:10g.
4. the method for a kind of silicon carbide ceramics surface vacuum deposited metals coating according to claim 1, it is characterized in that described vacuum cladding temperature is 1300 ~ 1400 DEG C, and soaking time is: 10 ~ 30 min.
5. the method for a kind of silicon carbide ceramics surface vacuum deposited metals coating according to claim 1, is characterized in that vacuum tightness≤4 × 10 in described vacuum oven
-2pa.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105367128A (en) * | 2015-11-27 | 2016-03-02 | 常熟市银洋陶瓷器件有限公司 | Preparation process suitable for metallization by bonding copper on aluminium oxide ceramic surface |
| CN109071364A (en) * | 2016-06-13 | 2018-12-21 | 株式会社Ihi | Ceramic matrix composite component and preparation method thereof |
| CN110714198A (en) * | 2019-09-11 | 2020-01-21 | 福建工程学院 | Method for preparing coating by laser cladding through vacuum sintering method |
| CN114605170A (en) * | 2022-04-13 | 2022-06-10 | 北航（四川）西部国际创新港科技有限公司 | Infiltration agent with multilayer coating structure and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261886A (en) * | 2014-09-24 | 2015-01-07 | 江苏大学 | Method for vacuum cladding of metal coating on surface of silicon carbide |
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2014
- 2014-10-22 CN CN201410564436.3A patent/CN104402533A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261886A (en) * | 2014-09-24 | 2015-01-07 | 江苏大学 | Method for vacuum cladding of metal coating on surface of silicon carbide |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105367128A (en) * | 2015-11-27 | 2016-03-02 | 常熟市银洋陶瓷器件有限公司 | Preparation process suitable for metallization by bonding copper on aluminium oxide ceramic surface |
| CN109071364A (en) * | 2016-06-13 | 2018-12-21 | 株式会社Ihi | Ceramic matrix composite component and preparation method thereof |
| CN110714198A (en) * | 2019-09-11 | 2020-01-21 | 福建工程学院 | Method for preparing coating by laser cladding through vacuum sintering method |
| CN110714198B (en) * | 2019-09-11 | 2022-03-08 | 福建工程学院 | Method for preparing coating by laser cladding through vacuum sintering method |
| CN114605170A (en) * | 2022-04-13 | 2022-06-10 | 北航（四川）西部国际创新港科技有限公司 | Infiltration agent with multilayer coating structure and preparation method thereof |
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Application publication date: 20150311 |